1JCL

OBSERVATION OF COVALENT INTERMEDIATES IN AN ENZYME MECHANISM AT ATOMIC RESOLUTION

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	SSRL BEAMLINE BL9-2
Synchrotron site	SSRL
Beamline	BL9-2
Temperature [K]	97
Detector technology	CCD
Collection date	2000-03-05
Detector	ADSC QUANTUM 4
Wavelength(s)	1.0
Spacegroup name	P 1 21 1
Unit cell lengths	48.540, 41.950, 144.980
Unit cell angles	90.00, 98.36, 90.00

Refinement procedure

Resolution	10.000 - 1.050
R-factor	0.143
R-free	0.16900
Structure solution method	FOURIER SYNTHESIS
Starting model (for MR)	native DERA
RMSD bond length	0.014
RMSD bond angle	0.029
Data reduction software	DENZO
Data scaling software	SCALEPACK
Refinement software	SHELXL-97

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	30.000	1.070
High resolution limit [Å]	1.050	1.050
Rmerge	0.063 *	0.667 *
Total number of observations	638223 *
Number of reflections	256887
<I/σ(I)>	14.8	1
Completeness [%]	95.5	64
Redundancy	2.5

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	unknown *	5.5	4 *	MPEG 5000, pH 5.5, VAPOR DIFFUSION, SITTING DROP, temperature 277K

Crystallization Reagents in Literatures

ID	crystal ID	solution	reagent name	concentration (unit)	details
1	1	1	enzyme	10-15 (mg/ml)
2	1	2	MPEG5000	13-18 (%)
3	1	2	cacodylate	0.1 (M)
4	1	2	glycerol	15-20 (%)